电感耦合等离子体原子发射光谱法测定钢铁及合金中析出相组成成分的研究

Study on determination of the compositions of precipitated phases in iron,steel and alloy by inductively coupled plasma atomic emission spectrometry

通过电感耦合等离子体原子发射光谱法(ICP-AES)测定了钢铁及合金析出相中Fe,Ni,Cr,Co,Mo,V,Ti,Mn,Al,Zr,W,Nb共12种组成成分。对仪器测量条件如功率、雾化器压力、进样量、积分时间进行了优化,对基体效应的影响、分析谱线的光谱干扰及其校正以及析出相的溶解条件进行了研究。通过调整电解量及试液稀释体积,控制试液中各元素的浓度在10 mg/mL以内,同时采用内标法有效地消除了基体干扰;通过选择合适的分析谱线,使各待测元素在测定范围内无明显光谱重叠干扰。主量元素对微痕量元素测定的背景干扰,可采用离峰扣背景校正法消除。采用盐酸、硝酸和氢氟酸溶解样品,既保证样品溶解完全,又使仪器测定具有较高的灵敏度和稳定性。用本法测定析出相中各组成元素,测定结果与经典的化学分析法的测定值具有很好的一致性,测定的相对标准偏差(RSD)均小于5%。

Twelve elements i.e. Fe, Ni, Cr, Co, Mo, V, Ti, Mn, Al, Zr, W and Nb in precipitated phase in iron, steel and alloy were determined by inductively coupled plasma-atomic emission spectrometry （ICP-AES）. The operation parameters of the instrument such as RF power, nebulizer pressure, sample introduction quantity and integration time were optimized. The influence of matrix effect, spectral interference and dissolving condition of precipitated phases were studied. The matrix effect can be removed by changing amount of electrolyzed sample, controlling each element in the test solution within the concentration level of 10 mg/mL and adding the internal standard. There is no apparent spectral interference for measured elements in the determination scope after appropriate analytical lines are selected. The background interference of major elements on micro elements can be removed by background correction method. Hydrochloric acid, nitric acid and hydrofluoric acid were used to dissolve precipitated phase samples in order to enable the samples to dissolve completely and the sensitivity and stability of determination to be higher. The analytical results of the method were in good agreement with those of chemical method and the relative standard deviations were below 5%.